高效分子排阻色谱法测定头孢克肟颗粒中聚合物的含量

目的建立高效分子排阻色谱法(HPSEC)测定头孢克肟颗粒中高分子聚合物的方法。方法采用HPLC,色谱柱为TSKgel G2000 SWXL(7.8 mm×300 mm,5μm),以磷酸盐缓冲液-乙腈(95∶5)为流动相,流速为0.6 mL·min^-1,柱温为20℃,检测波长为254 nm,进样体积为20μL。结果高分子聚合物峰与头孢克肟峰能有效分离,辅料无干扰,头孢克肟主峰的线性范围为0.153~20.635μg·mL^-1(r=0.9999),检测限为0.05μg·mL^-1,定量限为0.15μg·mL^-1;方法中样品测定的重复性(RSD=0.5%)与精密度(RSD=1.4%)良好;供试品溶液和对照品溶液,25℃条件下24 h保持稳定。微调方法中的流速、柱温和流动相比例,对检测结果无影响。结论此方法简便,耐用性好,灵敏度高,重复性好,可用于头孢克肟颗粒中高分子聚合物的含量检测。

Determination of the Polymers in Cefixime Granules by HPSEC

OBJECTIVE To establish a high performance size exclusion chromatography(HPSEC)method for the determination of the polymers in cefixime granules.METHODS HPLC was used by using TSKgel G2000 SWXL(7.8 mm×300 mm,5μm).The mobile phase was phosphate buffer-acetonitrile(95∶5).The flow rate was 0.6 mL·min^-1,the column temperature was 20℃,the detection wavelength was 254 nm,the injection volume was 20μL.RESULTS The polymers could be separated from cefixime well.The accessories made no interference.The linear of cefixime was within 0.153-20.635μg·mL^-1(r=0.9999).The limit of detection was 0.05μg·mL^-1,and the limit of quantification was 0.15μg·mL^-1.The repeatability(RSD=0.5%)and intermediate precision(RSD=1.4%)were fine.The sample solution and reference solution were stable at 25℃within 24 h.The robustness was well,when the flow rate,column temperature and mobile phase ratio were adjusted slightly,the result would not be affected.CONCLUSION This method is simple,robust,sensitive and repeatable.It can be used for quality control of the polymers in cefixime granules.